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分析测试中溶液体积测量的不确定度评定 总被引:3,自引:0,他引:3
对环境温度与溶液体积变动性的关系进行阐述.不确定度评定中要正确区分温度对容量器皿容积和对溶液体积的影响.溶液体积变动性的不确定度应根据其配制后温度的变化来评定,与容量器皿的校正温度无直接关系.文中对溶液体积不确定度评定中一些误区进行深入讨论. 相似文献
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化学计量测试简单地说是为了不同的目的而采用不同的方法来确定测试结果的不确定度的方法,这些方法是多种多样的。因此对测试不确定度因素的分析也比较困难。另一方面确定不确定度的方法与测定结果的不确定度并不是一种简单直接的关系。论述了参照某一标准进行的小型测试的不确定度,也对一般性测试的实例进行了介绍。 相似文献
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探讨了用原子吸收光谱法测定铜阳极泥中铋的不确定度的评定,阐述了测量结果不确定度主要来源于样品称量、试液定容体积和测量试液中铋的浓度产生的不确定度,计算了这些不确定的分量,最后计算出合成标准不确定度和扩展不确定度.通过评估,得出影响铋量测量不确定度的主要因素是测量试液中铋浓度时所引起的不确定度. 相似文献
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建立了电感耦合等离子体发射光谱(ICP-AES)测定糖果中铅的相应数学模型, 对数学模型中各个参数进行不确定度来源分析, 分别对A类不确定度或B类不确定度进行评定. 对各不确定度分量合成和扩展, 得到铅质量分数的不确定度. 结果表明: 标准溶液的配制、标准曲线拟合线性方程及样品溶液的定容是不确定度的主要来源. 相似文献
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氢化物原子荧光光谱法测定土壤中的汞的不确定度评定 总被引:1,自引:0,他引:1
对氢化物原子荧光光谱法测定土壤中汞含量的不确定度进行了评定.根据其测定方法和测定程序,分析了产生不确定度的重要因素.通过不确定度评定得出不确定度分量的主要来源为样品制备过程带来的不确定度.其中,样品消解产生的不确定度最大,最小二乘法拟合校准曲线校准所产生的不确定度次之;而标准溶液稀释及样品重复性产生的不确定度较以上二者小很多. 相似文献
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化学计量计量测试简地说是为了不同的目的而采用不同的方法来确定测试结果的不确定度的方法,这些方法是多种多样的。因此对测试不确定度因素的分析也比较困难。另一方面确定不确定度的方法与测定结果的不确定度并不是一种简单直接的关系。论述了参照某一标准进行的小型测试的不确定度,也对一般性测试的实例进行了介绍。 相似文献
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利用Kragten数值方法对医学检验中血清淀粉酶(amylase, AMY)活性浓度测量模型的合成标准不确定度(uc)进行计算,得到的结果与基于不确定度传播率的方法(GUM)基本一致,方法间计算的偏差均来自与该测量模型输出量呈非线性的输入量的贡献.推导出了非线性输入量引入的不确定度分量的解析式,表明Kragten法和含一阶项的GUM法计算结果的相对偏差仅与各输入量的相对不确定度呈函数关系.考查了逐渐增大的样品体积相对不确定度值(u(VS)/VS)对Kragten法计算的uc影响趋势,并与GUM法进行了比较.当相对不确定度的值增大而使测量结果非线性地取决于1个或多个输入量时,Kragten法仅给出了估计的标准不确定度,此时GUM法中的高阶项部分不应该被忽略.本研究对将Kragten法用于此类非线性模型的不确定度的评估,具有一定的参考和指导意义. 相似文献
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用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%. 相似文献
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Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction
Laurent Gavara Thomas Boisse Jean-Pierre Hénichart Adam Daïch Philippe Gautret 《Tetrahedron》2010,66(38):7544-5571
In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments. 相似文献
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Uroš Grošelj Mojca Žorž Amalija Golobič Branko Stanovnik Jurij Svete 《Tetrahedron》2013,69(52):11092-11108
A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives. 相似文献
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The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp3)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp2)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp2)?H and aliphatic 1,5- and 1,6-C(sp3)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp3)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp2)?H insertion. 相似文献
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The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula. 相似文献
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KMnO4-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields. 相似文献
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Rebecca J. Burton Mandy L. CrowtherNeal J. Fazakerley Shaun M. FilleryBarry M. Hayter Jason G. KettleCaroline A. McMillan Paula PerkinsPeter Robins Peter M. SmithEmma J. Williams Gail L. Wrigley 《Tetrahedron letters》2013
The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines. 相似文献
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N. A. Nedolya 《Chemistry of Heterocyclic Compounds》2008,44(10):1165-1219
The review contains a concise historical account and information on the most significant researches undertaken by the staff
at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry
of Heterocyclic Compounds.
Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee.
Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008. 相似文献
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N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%). 相似文献
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Shashikant U. Dighe Surya K. Samanta Shivalinga Kolle Sanjay Batra 《Tetrahedron》2017,73(17):2455-2467
An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y1 and Y2. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones. 相似文献